EP1425249B1 - Verfahren zur herstellung einer stabförmigen vorform sowie aus einer derartigen vorform hergestellte lichtleitfasern - Google Patents

Verfahren zur herstellung einer stabförmigen vorform sowie aus einer derartigen vorform hergestellte lichtleitfasern Download PDF

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Publication number
EP1425249B1
EP1425249B1 EP02753303A EP02753303A EP1425249B1 EP 1425249 B1 EP1425249 B1 EP 1425249B1 EP 02753303 A EP02753303 A EP 02753303A EP 02753303 A EP02753303 A EP 02753303A EP 1425249 B1 EP1425249 B1 EP 1425249B1
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EP
European Patent Office
Prior art keywords
substrate tube
bar
fluor
shaped preform
interior
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP02753303A
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English (en)
French (fr)
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EP1425249A1 (de
Inventor
Dennis Robert Simons
Arnold Bloemendal
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Draka Fibre Technology BV
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Draka Fibre Technology BV
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Publication date
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Publication of EP1425249A1 publication Critical patent/EP1425249A1/de
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Anticipated expiration legal-status Critical
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • C03B37/01853—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
    • C03B37/01815—Reactant deposition burners or deposition heating means
    • C03B37/01823—Plasma deposition burners or heating means
    • C03B37/0183—Plasma deposition burners or heating means for plasma within a tube substrate
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/08—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant
    • C03B2201/12—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant doped with fluorine
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
    • C03B2201/31—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with germanium

Definitions

  • the present invention relates to a method for manufacturing a bar-shaped preform, which method comprises the following steps:
  • the present invention further relates to a method for manufacturing optical fibres, using such a bar-shaped preform.
  • a PCVD (Plasma Coating Vapor Deposition) process is used for manufacturing internally clad glass tubes from which optical fibres are drawn, which tubes consists of a core and a jacket of glass, which core and which jacket have different refractive index values.
  • a hydrogen-free fluor compound is generally supplied to the hollow substrate tube. The addition of such a fluor compound prevents the incorporation of OH-groups during the PCVD process.
  • the incorporation of fluor in the glass structure causes the refractive index value of the glass to decrease, however. Said decrease is subsequently compensated by adding to the reactive gas mixture a component which has properties that cause the refractive index to increase, for example GeO 2 .
  • a component which has properties that cause the refractive index to increase for example GeO 2 .
  • One drawback of such a method is the fact that it leads to an increase of the total amount of dopes in the glass structure, resulting in an undesirable attenuation increase caused by the so-called Rayleigh scattering.
  • the object of the present invention is to provide a method for manufacturing a bar-shaped preform, from which preform optical fibres can be drawn, in which the incorporation of OH-groups in the glass layers is prevented in such a manner that said prevention will not take place at the expense of an increase of the Rayleigh scattering, which scattering is caused by an increase in the amount of dopes.
  • Another object of the present invention is to provide a method for manufacturing a bar-shaped preform, from which preform optical fibres can be drawn, the goal being a decrease of the attenuation peak at 1385 nm without this decrease leading to an increase of the attenuation in the rest of the spectrum.
  • the method as referred to in the introduction is characterized in that the amount of fluor compound that is supplied to the interior of the substrate tube in accordance with step i) is increased by a value of at least 10% at the end of the deposition of glass layers on the inner side of the substrate tube in accordance with step ii), after which the substrate tube is subjected to a heat treatment under conditions such that diffusion of the additionally incorporated fluor from the deposited glass layers will occur.
  • step iii) can be carried out in such a manner that the additionally incorporated fluor compound will diffuse from the deposited layers. It should be understood that fluor will be incorporated in the glass layers, so that fluor will exit when the intended diffusion takes place. This makes it possible to reduce the attenuation caused by the presence of OH-groups without the attenuation undesirably increasing due to Rayleigh scattering.
  • step iii) The heat treatment in accordance with step iii) is carried out in such a manner that the additional amount of fluor compound will diffuse from the deposited layers, which preferably takes place by slightly reducing the temperature that is used during the contraction step in comparison with the temperature that is conventionally used, with the heat treatment in addition being carried out for a slightly longer period of time than usual. Because the additional amount of fluor compound diffuses from the deposited layers during the contraction treatment, there is no need to carry out an additional compensation step comprising the usual additional supplying of one of more dopes which increase the refractive index.
  • the diffusion step it is in particular preferable for the diffusion step to take place before the contraction in accordance with step iii) is carried out.
  • the interior of the substrate tube is washed with an oxygen-containing gas.
  • the diffusion process that is used in the present invention can be realised by means of a stationary oven which fully envelopes the substrate tube, but in specific embodiments it is desirable to use an oven or other heat source which is movable along the length of the substrate tube.
  • step iii) it is in particular preferable to carry out the contraction according to step iii) by using an electric oven, in particular an electric resistance oven or induction oven, which oven in particular provides proper heating of the substrate tube to be contracted.
  • an electric oven in particular an electric resistance oven or induction oven, which oven in particular provides proper heating of the substrate tube to be contracted.
  • the supplying of the additional amount of fluor compound proportionally to a value at least 10%, preferably at least 20%, in excess of the amount of fluor compound that is usually supplied.
  • Suitable fluor compounds include in particular the hydrogen-free fluor-containing compounds, preferably volatile organic fluor-containing hydrocarbon compounds, such as CF 4 and C 2 F 6 , but inorganic fluor containing compounds, such as SiF 4 , can be used too, with the use of C 2 F 6 being preferred, since a distinct effect can already be observed when a small amount thereof is used.
  • the present invention furthermore relates to a method for manufacturing an optical fibre, which method is characterized in that the bar-shaped preform obtained in accordance with the method as described above is used.
  • the appended figure schematically shows the spectral attenuation gradient which is typical of an optical fibre. It should be understood that the appended figure merely functions to explain the present invention and should by no means construed as constituting a limitation of the scope thereof. The figure shows the three situations, viz.
  • an optical fibre obtained from a preform according to the prior art in which no special measures have been taken to reduce the characteristic peak at 1385 nm
  • an optical fibre in which an additional amount of fluor compound has been added during the PCVD process in a conventional manner, as a result of which the additional amount of fluor compound has been incorporated in the optical glass fibre in which embodiment the reduction of the refractive index that results from said additionally incorporated amount of fluor compound is compensated by the simultaneous incorporation of a dope which increases the refractive index, such as GeO 2 , in order to thus maintain the refractive index of the light-conducting core at a value equal to the value as measured in situation (1)
  • an optical 1 fibre obtained from a preform manufactured in accordance with the present method in which an additional amount of fluor compound has been added to the interior of the substrate tube during the PCVD process, and in which fluor has subsequently been removed from the deposited glass layers by diffusion.
  • a bar-shaped preform was manufactured in accordance with a usual method, and at the end of the process of depositing glass layers on the inner side of the substrate in accordance with step ii) the amount of fluor compound added to the interior of the substrate tube in accordance with step i) was increased by a value of at least 10%, after which the substrate tube was subjected to a heat treatment under conditions such that diffusion of the additionally incorporated fluor from the deposited glass layers occurred.
  • the measured attenuation decrease in comparison with the attenuation decrease in a standard optical fibre ranged from about -0.09 to about -0.12 dB/km.
  • Example 2 The same operations as in Example 1 were carried out, with this difference that 20% extra freon (C 2 F 6 ) was added.
  • the measured attenuation decrease in comparison with the attenuation decrease in a standard optical fibre ranged from about -0.20 to about -0.25 dB/km.
  • Example 2 The same operations as in Example 1 were carried out, except that 5% extra freon (C 2 F 6 ) was added.
  • the measured attenuation decrease in comparison with the attenuation decrease in a standard optical fibre ranged from about 0 to about -0.07 dB/km.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)
  • Treatment Of Fiber Materials (AREA)

Claims (11)

  1. Verfahren zur Herstellung einer stabförmigen Vorform, wobei das Verfahren die folgender "Schritte umfasst:
    i) Zuführen eines oder mehrerer reaktiver Gase, die dotiert oder nicht dotiert sein können, in das Innere eines Substratrohrs,
    ii) Durchführen einer Abscheidungsreaktion der Gase aus Schritt i) in dem Substratrohr, um eine oder mehrere Glasschichten auf der Innenseite des Substratrohrs zu erhalten, und
    iii) Kontrahieren des Substratrohrs aus Schritt ii), wobei das Rohr erwärmt wird, um die massive stabförmige Vorform zu erhalten,
    dadurch gekennzeichnet, dass
    die Menge der Fluorverbindung, die dem Inneren des Substratrohrs gemäß Schritt i) zugefühtt wird, am Ende der Abscheidung der Glasschichten auf der Innenseite des Substratrohrs gemäß Schritt ii) um einen Wert von mindestens 10% erhöht wird, woraufhin das Substratrohr einer Wärmebehandlung unter solchen Bedingungen unterzogen wird, dass Diffusion des zusätzlich eingeführten Fluors aus den abgeschiedenen Glasschichten stattfindet.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass der Diffusionsschritt stattfindet, bevor die Kontraktion gemäß Schritt iii) durchgeführt wird.
  3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, dass der Wärmebehandlungsschritt bei einer Temperatur unter dem Erweichungspunkt des Substratrohrs während dies Diffusionsschritts durchgeführt wird.
  4. Verfahren nach einem oder mehreren der Ansprüche 2 bis 3, dadurch gekennzeichnet, dass das Substratrohr während des Diffusionsschritts unter einem inneren Druck gehalten wird, um das Kontrahieren des Substratrohrs zu verhindern.
  5. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass der Diffusionsschritt während der Kontraktion gemäß Schritt iii) stattfindet.
  6. Verfahren nach einem oder mehreren der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass das Innere des Substratrohrs während des Diffusionsschritts mit einem sauerstoffhaltigen Gas gewaschen wird.
  7. Verfahren nach einem oder mehreren der vorstehenden Ansprüche, dadurch gekennzeichnet, dass ein elektrischer Ofen in Schritt iii) verwendet wird.
  8. Verfahren nach einem oder mehreren der vorstehenden Ansprüche, dadurch gekennzeichnet, dass das Zuführen der zusätzlichen Menge an Fluorverbindung proportional durchgeführt wird.
  9. Verfahren nach einem oder mehreren der vorstehenden Ansprüche, dadurch gekennzeichnet, dass das Zuführen der erhöhten Menge an Fluorverbindung in das Innere dies Substratrohrs am Ende von Schritt ii) nicht durch das gleichzeitige Zuführen von einem oder mehreren Bestandteilen, welche den Brechungsindex erhöhen, kompensiert wird.
  10. Verfahren nach einem oder mehreren der vorstehenden Ansprüche, dadurch gekennzeichnet, dass C2F6 als Fluorverbindung verwendet wird.
  11. Verfahren zur Herstellung einer optischen Faser unter Verwendung einer stabförmigen Vorform, die durch Verwendung eines Verfahrens nach einem oder mehreren der Ansprüche 1 bis 10 erhalten wurde.
EP02753303A 2001-09-13 2002-08-28 Verfahren zur herstellung einer stabförmigen vorform sowie aus einer derartigen vorform hergestellte lichtleitfasern Expired - Lifetime EP1425249B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
NL1018951A NL1018951C2 (nl) 2001-09-13 2001-09-13 Werkwijze voor het vervaardigen van een staafvormig vormdeel alsmede een werkwijze voor het uit een dergelijk staafvormig vormdeel vervaardigen van optische vezels.
NL1018951 2001-09-13
PCT/NL2002/000564 WO2003022760A1 (en) 2001-09-13 2002-08-28 A method for manufacturing a bar-shaped preform as well as a method for manufacturing optical fibres from such a bar-shaped preform

Publications (2)

Publication Number Publication Date
EP1425249A1 EP1425249A1 (de) 2004-06-09
EP1425249B1 true EP1425249B1 (de) 2006-05-10

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EP02753303A Expired - Lifetime EP1425249B1 (de) 2001-09-13 2002-08-28 Verfahren zur herstellung einer stabförmigen vorform sowie aus einer derartigen vorform hergestellte lichtleitfasern

Country Status (9)

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US (1) US7092611B2 (de)
EP (1) EP1425249B1 (de)
JP (1) JP4350510B2 (de)
CN (1) CN1245342C (de)
AT (1) ATE325782T1 (de)
BR (1) BR0212381B1 (de)
DE (1) DE60211350T2 (de)
NL (1) NL1018951C2 (de)
WO (1) WO2003022760A1 (de)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL1032867C2 (nl) * 2006-11-14 2008-05-15 Draka Comteq Bv Inrichting en een werkwijze voor het uitvoeren van een depositieproces van het type PCVD.
NL2004544C2 (nl) * 2010-04-13 2011-10-17 Draka Comteq Bv Inwendig dampdepositieproces.
NL2004546C2 (nl) * 2010-04-13 2011-10-17 Draka Comteq Bv Inwendig dampdepositieproces.
NL1041529B1 (en) * 2015-10-16 2017-05-02 Draka Comteq Bv A method for etching a primary preform and the etched primary preform thus obtained.

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DE2538313C3 (de) * 1975-08-28 1981-11-05 Heraeus Quarzschmelze Gmbh, 6450 Hanau Verfahren zur Herstellung eines Vorproduktes für die Erzeugung eines optischen, selbstfokussierenden Lichtleiters
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JPS598634A (ja) * 1982-07-07 1984-01-17 Hitachi Cable Ltd 偏波面保存光フアイバ母材の製造法
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JPS63307136A (ja) * 1987-06-08 1988-12-14 Nippon Telegr & Teleph Corp <Ntt> 光ファイバ母材の製造方法
FR2620696B1 (fr) * 1987-09-22 1992-10-09 Comp Generale Electricite Procede de fabrication de fibre optique a coeur de silice entoure de silice fluoree
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JP3530676B2 (ja) * 1995-04-26 2004-05-24 キヤノン株式会社 光受容部材の製造方法、該光受容部材、該光受容部材を有する電子写真装置及び該光受容部材を用いた電子写真プロセス

Also Published As

Publication number Publication date
JP2005502575A (ja) 2005-01-27
CN1553881A (zh) 2004-12-08
BR0212381B1 (pt) 2010-11-30
DE60211350T2 (de) 2007-04-12
ATE325782T1 (de) 2006-06-15
US7092611B2 (en) 2006-08-15
EP1425249A1 (de) 2004-06-09
BR0212381A (pt) 2004-08-17
WO2003022760A1 (en) 2003-03-20
NL1018951C2 (nl) 2003-03-14
CN1245342C (zh) 2006-03-15
JP4350510B2 (ja) 2009-10-21
US20050081566A1 (en) 2005-04-21
DE60211350D1 (de) 2006-06-14

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